B22-Multimode InfraRed imaging And Microspectroscopy
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Diamond Proposal Number(s):
[31423]
Open Access
Abstract: A facile approach is demonstrated for synthesizing a mechanically tough ZIF-71 [Zn(dcIm)2; dcIm = 4,5-dichloroimidazole] monoliths with a polymer binder, employing namely poly-methyl methacrylate (PMMA) through a sol-gel process. The addition of a slight polymer binder (∼10 wt.%) to the sol-gel mixture is shown to enhance the mechanical properties such as the elastic modulus, hardness, fracture toughness, strain hardening, and creep behavior of the composite monoliths compared to the pure ZIF-71 monoliths. Nitrogen sorption measurements revealed that the composite monoliths have a high surface area (∼350 m2/g) although it was reduced from ∼600 m2/g due to pore blockage by the polymer. Composite monoliths exhibit less surface cracks and are relatively stiffer but are notably tougher than the pure ZIF-71 monoliths as the fracture toughness tripled from around 0.15 MPa m1/2 to around 0.45 MPa m1/2. Despite the incorporation of a small quantity of polymer in the monolith, this has a significant impact on increasing the mechanical stiffness, hardness and fracture resistance of the resulting monoliths. Creep response observed under a constant load revealed the presence of PMMA incorporated in the composite monolith. Nearfield infrared (IR) nanospectroscopy via nanoFTIR and pseudoheterodyne (PsHet) scattering-Scanning Nearfield Optical Microscopy (s-SNOM) IR imaging on plastically deformed and indented surfaces revealed local chemical structure-mechanical interactions. Our findings suggest that the polymer chains are trapped inside the ZIF-71 structure, thereby improving the mechanical resilience that might pave the way to future scaling up of MOF monoliths for practical applications and durable devices.
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Jan 2026
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B22-Multimode InfraRed imaging And Microspectroscopy
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Marta
Morana
,
Lorenzo
Barni
,
Haixing
Fang
,
Giulia
Marras
,
Gianfelice
Cinque
,
Antonio
Angellotti
,
Fabrizio
Nestola
,
Alla
Logvinova
,
Denis
Mikhailenko
,
Luca
Bindi
,
Vincenzo
Stagno
Diamond Proposal Number(s):
[35052]
Open Access
Abstract: The investigation of mineral inclusions in diamonds represents a unique tool to better understand the mineralogy and composition of hidden portions of Earth's mantle and, hence, determine conditions of pressure and temperature at the time of diamond formation. Using a combination of experimental techniques and different geothermobarometric approaches, we characterized a natural diamond from Udachnaya kimberlite pipe entrapping nine inclusions; the inclusions are five garnets, three clinopyroxene and one sulfide and represent an eclogitic paragenesis. Here, we adopted, for the first time, the elastic geobarometry method to the garnet-diamond inclusion-host system to calculate the entrapment conditions for the diamond-garnet pair, resulting in 5.7(±0.3) GPa at 1154 °C. These P-T data are compared with estimates obtained through chemical geothermobarometry, employing T projection onto the local geotherm, a common approach used for eclogite xenoliths in absence of robust calibrated barometers. Our data demonstrate that elastic geobarometry for the garnet-diamond pair results to be a very reliable tool to determine the diamond formation also for eclogitic systems and this will allow to expand our knowledge on eclogitic diamonds in terms of depth of formation.
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Nov 2025
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B22-Multimode InfraRed imaging And Microspectroscopy
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A.
Angellotti
,
M.
Morana
,
L.
Barni
,
G.
Cinque
,
Y.
Lu
,
R.
Tao
,
G.
Marras
,
A.
Logvinova
,
L.
Bindi
,
D.
Mikhailenko
,
V.
Stagno
Diamond Proposal Number(s):
[35052]
Open Access
Abstract: Natural diamonds are exceptional carriers of mineralogical and chemical information from inaccessible depths of our planet. During their crystallization, they can host light elements such as H and N preserving a natural archive of mantle chemistry that, in turn, allows a better understanding of the chemical composition of the growth media, mechanisms of their formation and residence temperatures in the interior of Earth. However, how N and H distribute near entrapped minerals is still unknown. In this study we investigated the effect of chromite mineral inclusions on the spatial distribution of nitrogen and hydrogen in two natural diamonds of peridotitic origin using in situ synchrotron-based Fourier transform infrared microspectroscopy. From the acquisition and optimization of high-resolution maps, we determined the distribution of nitrogen, hydrogen, and nitrogen aggregation state.
Our results reveal a dependence between the absorption of H-related peaks with the incorporation of pairs of nitrogen atoms (NA-centers). We explain it as indication that chemical interactions between chromite and H might be masked by variations in the N aggregation state. We also conclude that synchrotron micro-FTIR is an advanced technique to assist the synthesis of N- (and H-) doped diamonds for industrial applications.
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Nov 2025
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B22-Multimode InfraRed imaging And Microspectroscopy
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Lewis
Dowling
,
Charlotte
Evans
,
Paul
Roach
,
Lisa
Vaccari
,
Gianfelice
Cinque
,
Chiara Maria
Stani
,
Giovanni
Birarda
,
Vishnu Anand
Muruganandan
,
Srinivas
Pillai
,
Daniel Gey
Van Pittius
,
Apurna
Jegannathen
,
Josep
Sulé-Suso
Diamond Proposal Number(s):
[36088]
Abstract: Liquid biopsy is revolutionizing cancer management, with circulating tumor cells (CTCs), offering a transformative approach to screening, diagnosis, and treatment monitoring. However, existing CTC isolation methods relying on antigen expression or physical properties lack robustness, are operator-dependent, and suffer from automation challenges, leading to inconsistent and time-intensive analyses. A universal, unbiased methodology for CTC detection across tumor types is critically needed. Here, we present the first proof-of-concept study demonstrating the use of Fourier transform infrared (FT-IR) microspectroscopy to study cytospun blood samples coupled with a random forest (RF) classifier, for the detection of a single CTC in the blood of a lung cancer patient as confirmed via immunohistochemistry. Notably, our method utilizes glass coverslips as substrates, routinely employed in pathology departments, enabling seamless integration with histopathological analyses (e.g., staining, immunohistochemistry). Using FT-IR spectral data from in vitro growing lung cancer cells as a training model, we achieved precise CTC identification based on biochemical composition, specifically within the Fingerprint region (1800 cm–1 to 1350 cm–1). This study introduces FT-IR microspectroscopy as a novel, label-free approach for CTCs detection in liquid biopsies, with the potential to redefine cancer diagnostics. By enhancing precision and accessibility in CTC identification, the clinical implementation of this methodology may represent a significant advancement in personalized oncology, offering a clinically viable tool for real-time cancer monitoring and improved patient stratification.
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Oct 2025
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B22-Multimode InfraRed imaging And Microspectroscopy
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Diamond Proposal Number(s):
[30369]
Open Access
Abstract: Metal–organic framework (MOF) materials have demonstrated promising potential as triboelectric nanogenerators (TENGs) in recent studies due to their unique advantages, such as high surface area and vast tunability in physicochemical response. However, the poor mechanical stability and durability of MOF-based TENGs may limit their practical applications. In this study, a MOF-based, noncontact rotational TENG has been designed using a highly fluorinated MOF, namely, ZIF-8-CF3, incorporated into a poly(vinylidene fluoride) (PVDF) polymer matrix to enhance triboelectric output and mitigate material abrasion during operation. The noncontact TENG demonstrated excellent voltage and current output of 280 ± 8 V and 19.0 ± 0.4 µA, respectively. The power density of the prepared noncontact TENG based on the composite is ∼66 µW/cm2, about 2 times higher than that of the neat PVDF-based TENG. The noncontact TENG exhibits excellent mechanical stability, sustaining high triboelectric output over a test comprising half a million cycles. The potential application of the ZIF-8-CF3/PVDF-based TENG was tested by powering various microelectronics under rotational operations. The prepared rotational device also shows strong potential for use in force and humidity sensing. The basic mechanism of the ZIF-8-CF3/PVDF-based TENG was revealed by ab initio quantum mechanical modeling and nanoscale surface potential analysis.
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Sep 2025
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B22-Multimode InfraRed imaging And Microspectroscopy
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Diamond Proposal Number(s):
[20377]
Abstract: Myopathies, a group of muscle disorders with varied etiologies, cause significant alterations in muscle tissue biomolecular composition. Accurate differentiation of myopathies is essential for effective diagnosis, treatment and prognosis. Fourier-transform infrared microspectroscopy (microFTIR) is a valuable, non-destructive method for analysing the main biological macromolecules at the microscopic level. Therefore, it may offer insight into the investigation of both primary and secondary myopathies. In our work we use microFTIR to identify unique spectral markers associated with disease progression. For this purpose, muscle tissues from patients diagnosed with dystrophy and myopathy, as well as control tissues, were subjected to probing. The results reveal significant differences in the distribution of lipid, protein, and nucleic acid absorption bands among the sample groups, particularly in regions associated with muscle fibre and connective tissue structure. Notably, vibrational bands at ∼1043, 1388, and 2873 cm−1 assigned to nucleic acids, fatty acids and lipids, respectively showed highest discriminative power in distinguishing pathological from control tissues. In addition, the use of synchrotron radiation FTIR microspectroscopy enabled precise analysis of endomysium-specific changes. This work demonstrates the potential of microFTIR as a novel diagnostic tool for myopathy, offering an early-stage insight into muscle degradation that can support histopathological diagnosis. The ability of microFTIR to detect subtle biomolecular changes represents a promising step forward in non-invasive diagnostics of muscle disorders.
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Jul 2025
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B22-Multimode InfraRed imaging And Microspectroscopy
I19-Small Molecule Single Crystal Diffraction
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Open Access
Abstract: The latest developments in acoustic technology and their integration of standing waves offers the potential to eject and trap tiny amounts of both liquid and solids with precision and stability in free space. This is appealing for experimenters at Light Sources who are traditionally relying on the use of containers or on the manual attachment of the samples to solid supports for analysis with X rays or IR. Here we present a brief overview of applications of acoustics and levitation for sample manipulation and delivery currently under investigation at Diamond Light source.
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May 2025
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B22-Multimode InfraRed imaging And Microspectroscopy
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Diamond Proposal Number(s):
[27207]
Open Access
Abstract: There is cumulative evidence that lipid metabolism plays a key role in the pathogenesis of various neurodegenerative disorders including Alzheimer’s disease (AD). Visualising lipid content in a non-destructive label-free manner can aid in elucidating the AD phenotypes towards a better understanding of the disease. In this study, we combined multiple optical molecular-specific methods, Fourier transform infrared (FTIR) spectroscopic imaging, synchrotron radiation-infrared (SR-IR) microscopy, Raman and stimulated Raman scattering (SRS) microscopy, and optical-photothermal infrared (O-PTIR) microscopy with multivariate data analysis, to investigate the biochemistry of brain hippocampus in situ using a mouse model of tauopathy (rTg4510). We observed a significant difference in the morphology and lipid content between transgenic (TG) and wild type (WT) samples. Immunohistochemical staining revealed some degree of microglia co-localisation with elevated lipids in the brain. These results provide new evidence of tauopathy-related dysfunction in a preclinical study at a subcellular level.
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Oct 2024
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B22-Multimode InfraRed imaging And Microspectroscopy
I24-Microfocus Macromolecular Crystallography
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Diamond Proposal Number(s):
[31420, 32898, 37199]
Open Access
Abstract: Hemoglycin, a space polymer of glycine and iron, has been identified in the carbonaceous chondritic meteorites Allende, Acfer 086, Kaba, Sutter's Mill and Orgueil. Its core form has a mass of 1494 Da and is basically an antiparallel pair of polyglycine strands linked at each end by an iron atom. The polymer forms two- and three- dimensional lattices with an inter-vertex distance of 4.9 nm. Here the extraction technique for meteorites is applied to a 2.1 Gya fossil stromatolite to reveal the presence of hemoglycin by mass spectrometry. Intact ooids from a recent (3000 Ya) stromatolite exhibited the same visible hemoglycin fluorescence in response to x-rays as an intact crystal from the Orgueil meteorite. X-ray analysis confirmed the existence in ooids of an internal three-dimensional lattice of 4.9 nm inter-vertex spacing, matching the spacing of lattices in meteoritic crystals. FTIR measurements of acid-treated ooid and a Sutter's Mill meteoritic crystal both show the presence, via the splitting of the Amide I band, of an extended anti-parallel beta sheet structure. It seems probable that the copious in-fall of carbonaceous meteoritic material, from Archaean times onward, has left traces of hemoglycin in sedimentary carbonates and potentially has influenced ooid formation.
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Oct 2024
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B22-Multimode InfraRed imaging And Microspectroscopy
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Diamond Proposal Number(s):
[26320]
Open Access
Abstract: The cellular response to cisplatin was assessed in human osteosarcoma cells, using synchrotron-based (SR) Fourier Transform InfraRed nanospectroscopy (nano-FTIR) at the MIRIAM beamline B22 of Diamond Light Source (UK). This label-free mapping method delivered simultaneous morphological and biochemical information on a subcellular level (i.e. 100 s nanometer or better). Based on specific spectral biomarkers, the main biochemical constituents affected by the drug were identified at distinct locations within the cell´s inner body. Cisplatin was shown to have a noteworthy effect on proteins, mostly within the cytoplasm. A clear drug impact on cellular lipids was also observed. Within current literature on s-SNOM, this nanospectroscopy work represents a first successful application in life sciences providing full fingerprint nano-FTIR spectra across intact human cancer cells.
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Jul 2024
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